Resonance Spectra Research Articles

Synthesis, docking study, and antitumor evaluation of benzamides and oxadiazole derivatives of 3-phenoxybenzoic acid as VEGFR-2 inhibitors.

Current chemotherapeutic agents have several limitations, including lack of selectivity, the development of undesirable side effects, and chemoresistance. As a result, there is an unmet need for the development of novel small molecules with minimal side effects and the ability to specifically target tumor cells. A new series of 3-phenoxybenzoic acid derivatives, including 1,3,4-oxadiazole derivatives (4a-d) and benzamides derivatives (5a-e) were synthesized; their chemical structures were confirmed by Fourier-transform infrared spectroscopy, 1H nuclear magnetic resonance (NMR), 13C NMR, and mass spectra; and various physicochemical properties were determined. The antiproliferative activities of the new derivatives were evaluated by means of the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. Three compounds (4b, 4c, and 4d) exhibited cytotoxicity against two of the three cell lines tested, five compounds (3, 4a, 5a, 5b, and 5e) were toxic to one cell line, while two compounds (5c and 5d) were not cytotoxic to any of the three cell lines tested in the current study. Based on docking scores, MTT assay findings, and vascular endothelial growth factor receptor 2 (VEGFR-2) kinase activity data, Compound 4d was selected for further biological investigation. Flow cytometry was used to determine the mode of cell death (apoptosis vs. necrosis) and the effect on cell cycle progression. Compound 4d arrested HepG2 hepatocellular carcinoma cells in the G2/M phase and activated both the intrinsic and extrinsic apoptosis pathways. In conclusion, Compound 4d has shown promising results for future research as a potent VEGFR-2 tyrosine kinase inhibitor.

Donor-acceptor covalent organic framework/ZnIn2S4 core-shell structure S-scheme heterostructure for efficient photocatalytic hydrogen evolution

Covalent organic frameworks (COFs) show promising prospect as the photocatalysts with advantages of exceptional light adsorption capability, large specific surface area, and adjustable band structure. However, COFs usually suffer from severe recombination of photogenerated carriers. Therefore, there is an urgent demand to design effective COF-based heterostructures to enhance the separation of carriers. In this work, a porphyrin-based COF with electron donor-acceptor structure is synthesized via condensation polymerization by using 5,10,15,20-tetrakis(4-aminophenyl)porphyrin (TAPPP) and N,N,N',N'-tetra(4-formylphenyl)benzidin (NFPBD) as the donor and acceptor, respectively. Subsequently, ZnIn2S4 (ZIS) are successfully in-situ grown on the surface of porphyrin-based COF, forming a novel core-shell structure. The in-situ synthesized ZIS with positive charges can be easily adsorbed on the negatively charged sites of the COF’s surface via the electrostatic interaction. This organic/inorganic hybrid COF-ZIS heterostructure exhibits a superior photocatalytic hydrogen evolution (PHE) rate of 695 μmol g−1 h−1, approximately three times higher than that of ZIS. The construction of COF-ZIS heterostructure plays an important role in enhancing the separation and transport of photogenerated carriers, which provides more electrons at the surface of ZIS to take part in proton reduction. Electron paramagnetic resonance spectra confirm the charge carriers transfer mode in the COF-ZIS heterostructure via an S-scheme mechanism. Moreover, upon loading Pt as the cocatalyst, the heterostructure achieves an effective PHE rate of 2711 μmol g−1 h−1 along with an exceptional stability. Additionally, the COF-ZIS heterostructure reaches up to 2.45% of apparent quantum efficiency at 400 nm. Notably, the average lifetime of the COF-ZIS heterostructure increases by 43.2% and 98.9% compared to that of ZIS and the COF individually, as observed through single-particle fluorescence spectroscopy. This work gives valuable inspiration into the building of donor-acceptor COF-based S-scheme heterostructures to achieve highly effective green energy conversion by aligning band structures.

Modifying single-crystal silicon and trimming silicon microring devices by femtosecond laser irradiation

Single-crystal silicon (c-Si) is a vital component of photonic devices and has obvious advantages. Moreover, femtosecond-pulsed laser interactions with matter have been widely applied in micro/nanoscale processing. In this paper, we report the modification mechanisms of c-Si induced by a femtosecond laser (350 fs, 520 nm) at different pulse fluences, along with the mechanism of this technique to trim the phase error of c-Si-based devices. In this study, several distinct types of final micro/nanostructures, such as amorphization and ablation, were analyzed. The near-surface morphology was characterized using optical microscopy, scanning electron microscopy, and atomic force microscopy. The main physical modification processes were further analyzed using a two-temperature model. By employing Raman spectroscopy, we demonstrated that a higher laser fluence significantly contributes to the formation of more amorphous silicon components. The thickness of the amorphous layer was almost uniform (approximately 30 nm) at different induced fluences, as determined using transmission electron microscopy. From the ellipsometry measurements, we demonstrated that the refractive index increases for amorphization while the ablation decreases. In addition, we investigated the ability of the femtosecond laser to modify the effective index of c-Si microring waveguides by either amorphization or ablation. Both blue and red shifts of resonance spectra were achieved in the microring devices, resulting in double-direction trimming. Our results provide further insight into the femtosecond laser modification mechanism of c-Si and may be a practical method for dealing with the fabrication errors of c-Si-based photonic devices.

Characterization of anthranilic acid produced by Virgibacillus salarius MML1918 and its bio-imaging application.

Anthranilic acid (AA) holds significant importance in the chemical industry. It serves as a crucial building block for the amino acid tryptophan by manipulating the tryptophan biosynthesis pathway, it is possible to increase the production of anthranilic acid. In this study, we utilized metabolic engineering approaches to produce anthranilic acid from the halophilic bacterium Virgibacillus salarius MML1918. The halophilic bacteria were grown in an optimized production medium, and mass production of secondary metabolites was made in ATCC medium 1097 Proteose peptone-for halophilic bacteria and subjected to column chromatography followed by sub-column chromatography the single band for the purified compound was confirmed. Further, various spectral analyses were made for the partially purified compounds, and fluorescence microscopy for fungal cell observation was performed. The purified compound was confirmed by single crystal X-ray diffraction (XRD) analysis, and it was identified as 2-amino benzoic acid. The Fourier transform infrared Spectroscopy (FT-IR) spectrum and nuclear magnetic resonance (NMR) spectrum also confirm the structural characteristic of 2-amino benzoic acid. The UV-Vis absorption spectrum of AA shows the maximum absorption at 337.86nm. The emission spectrum of 2-amino benzoic acid showed the maximum emission at 453nm. The bio-imaging application of 2-amino benzoic acid was examined with fungal mycelium of Rhizoctonia solani. It was effectively bound and emitted the blue color at the concentration of 200 and 300µg/mL. The halophilic bacterium (V. salarius), may have unique metabolic pathways and requirements compared to non-halophilic organisms, to produce AA effectively. This could have implications for industrial biotechnology, particularly in manufacturing environments where high salt concentrations are present and also it can be used as bio-imaging agent.

Investigation the optical and structural properties of Mn-doped Sb2S3 nanocrystals embedded in host glass

The search for earth-abundant and non-toxic elements is essential for the manufacture of sustainable optical devices. In this context, dilute magnetic semiconductor (DMS) xMn-doped Sb2S3 nanocrystals (NCs) embedded in host glass were synthesized by the fusion method. Differential Thermal Analysis shows evidence of Sb2S3 phase crystallization peak and changes in glass transition and crystallization temperatures of the host glass with the presence of xMn-doped Sb2S3 NCs. Transmission electron microscopy images show the formation of xMn-doped Sb2S3 NCs with increasing size (2.1–3.8 nm) as a function of concentration (x = 0.00 to 0.40), respectively. X-ray diffraction measurements reinforced the evidence for the orthorhombic structure of xMn-doped Sb2S3 NCs embedded in glass. Energy dispersive X-ray spectroscopy analyses confirm the S, Sb and Mn precursor elements of DMS NCs. Atomic and magnetic force microscopy measurements show the magnetic contrast patterns resulting from the incorporation of Mn atoms into the Sb2S3 structure. The electronic paramagnetic resonance spectrum confirms the presence of Mn2+ ions (3d5) located in the crystal field of the Sb2S3 semiconductor due to six hyperfine transitions. The redshift of the Raman vibrational mode (1Ag) with increasing xMn concentration gives strong evidence for the presence of Mn2+ ions in sulfur vacancies (VS) in the Sb2S3 unit cell. Optical absorption and photoluminescence (PL) spectroscopy measurements for xMn-doped Sb2S3 NCs show the subtle tunable redshift of the band gap and excitonic recombination in the green-red region, with increasing x concentration. PL confirms that dopant Mn2+ ions fill VS2 that are dominant in Sb2S3. Therefore, the position of the energy states after the increasing concentration of Mn2+ dopant ions gives rise to insight into luminescence for future research scenarios and applications involving sustainable DMS NCs.

Preliminary analyses of radiophotoluminescence centers in a recently developed Ag-doped alkali-phosphate glass (SAPANS)

The mechanism behind radiophotoluminescence (RPL) emission in Ag-doped alkali-phosphate glass remains unclear. To contribute to resolving this issue, the authors measured and analyzed the temporal change of electron spin/paramagnetic resonance (ESR) spectrum of a recently developed, weather-resistant RPL glass, named “SAPANS,” after irradiation with X-rays. As a result, a continuous gradual increase in Ag2+-derived signals was observed even at four weeks post-irradiation, which corresponded well with the time build-up pattern of the RPL of SAPANS. In contrast, the signals derived from phosphorous-oxygen-hole centers (POHC) rapidly decreased over a few days. The peaks of Ag0 and Ag2+ were not successfully separated from the ESR spectra because of the possible overlap of unidentified peaks, which implies a complex mechanism of RPL-center formation in Ag-doped alkali-phosphate glass that requires further investigation.

Producing Conventional and Transient Amino(mercapto)methyl Radicals by Addition of Muonium to a Crystalline Thioformamide (Mes*NHCH=S).

Muonium (Mu=μ+e-) is composed of a muon of light isotope of proton (μ+) and electron (e-) and can be used as a light surrogate for a hydrogen atom. In this paper, we investigated addition of muonium to a newly synthesized Mes*-substituted thioformamide (Mes*NHCH=S, Mes*=2,4,6-tBu3C6H2). Transverse-field muon spin rotation (TF-μSR) of a solution sample of the thioformamide confirmed addition of muonium to the sulfur atom leading to the corresponding C-centered radical [Mes*NHC(H)⋅-SMu]. Density functional theory (DFT) calculations assigned a conventional amino(mercapto)methyl radical, in which both nitrogen and carbon were slightly pyramidalized, and the calculated muon hyperfine coupling constant (hfcc) including the muon isotope effect was compatible with the experimentally determined parameter. However, the muon level-crossing resonance (μLCR) spectrum of an anisotropic crystalline sample indicated two paramagnetic species, and the major product showed the considerably larger muon hfcc compared with the conventional structure of the amino(mercapto)methyl radical. The unusual transient muoniated thioformamide with the larger muon hfcc that showed rapid relaxation could be only explained by a transient structure including planarization of the nitrogen and carbon atoms in Mes*NHC(H)⋅-SMu.

Enhanced degradation of carbamazepine in water over Fe3O4@ZIF-8 nanocomposites with persulfate or peroxymonosulfate as activator

In this work, the Fe3O4@ZIF-8 catalyst was prepared by combining Fe3O4 with ZIF-8 for degrading carbamazepine (CBZ) in water, using activated persulfate (PS) and peroxymonosulfate (PMS). We investigated the optimal catalysts and reaction conditions for using PS or PMS as activators by varying the pH, temperature, catalyst dosage, as well as the dosage of PS and PMS, respectively. The results demonstrated that the CBZ removal rate using Fe3O4@ZIF-8 reached 98.1% after 30 min with a mass ratio of Fe3O4 to ZIF-8 = 3:1, temperature = 40°C, catalyst dosage = 0.50 g·L−1, and PS dosage = 0.25 g·L−1, using pH = 3.0. Characterization results show due to the fact that the presence of ZIF-8 facilitates the dispersion of the catalytic active species Fe3O4, prevents the agglomeration of the active species, increases the number of active species, and improves the catalytic performance. Furthermore, radical quenching assay and electron paramagnetic resonance spectra successfully identified the main oxidizing components generated in the system, namely SO4•− and •OH.

Mechanisms of acrylamide biosorption by Lactobacillus plantarum ATCC8014 peptidoglycan

This study extracted peptidoglycan (PG) from Lactobacillus plantarum ATCC8014, its acrylamide (AA) adsorption behavior was evaluated by creating adsorption models, and its binding characterizations were investigated by physicochemical methods. The kinetics and isothermal model revealed that the biosorption of AA by PG conformed to Langmuir, Freundlich equations, and the second-order kinetic model, confirming that the adsorption process involved both physisorption and chemisorption. Fourier transform infrared spectroscopy and chemical blocking of functional groups confirmed that carboxyl, amino and hydroxyl groups were involved. Meanwhile, a new peak was generated in the proton nuclear magnetic resonance spectrum of PG upon adsorption, and the water contact angle was significantly reduced, indicating that hydrogen bonds and hydrophobic force were involved in the biosorption. Besides, energy dispersive spectroscopy and X-ray photoelectron spectroscopy results have important findings, suggesting that amide bonds might be formed during the adsorption process. Subsequently, this speculation was confirmed by the identification results of amidase. Overall, our results indicated that the mechanism of adsorption is complex and involves hydrogen bonding, hydrophobic forces and the formation of chemical bonds.

Dual Structure of a Vanadyl-Based Molecular Qubit Containing a Bis(β-diketonato) Ligand.

We designed [VO(bdhb)] (1') as a new electronic qubit containing an oxovanadium(IV) ion (S = 1/2) embraced by a single bis(β-diketonato) ligand [H2bdhb = 1,3-bis(3,5-dioxo-1-hexyl)benzene]. The synthesis afforded three different crystal phases, all of which unexpectedly contain dimers with formula [(VO)2(bdhb)2] (1). A trigonal form (1h) with a honeycomb structure and 46% of solvent-accessible voids quantitatively transforms over time into a monoclinic solvatomorph 1m and minor amounts of a triclinic solventless phase (1a). In a static magnetic field, 1h and 1m have detectably slow magnetic relaxation at low temperatures through quantum tunneling and Raman mechanisms. Angle-resolved electron paramagnetic resonance (EPR) spectra on single crystals revealed signatures of low-dimensional magnetic behavior, which is solvatomorph-dependent, being the closest interdimer V···V separations (6.7-7.5 Å) much shorter than intramolecular V···V distances (11.9-12.1 Å). According to 1H diffusion ordered spectroscopy (DOSY) and EPR experiments, the complex adopts the desired monomeric structure in organic solution and its geometry was inferred from density functional theory (DFT) calculations. Spin relaxation measurements in a frozen toluene-d8/CD2Cl2 matrix yielded Tm values reaching 13 μs at 10 K, and coherent spin manipulations were demonstrated by Rabi nutation experiments at 70 K. The neutral quasi-macrocyclic structure, featuring nuclear spin-free donors and additional possibilities for chemical functionalization, makes 1' a new convenient spin-coherent building block in quantum technologies.

Thermo‐Optical Switches Based on Spin‐Crossover Molecules with Wideband Transparency

AbstractIn this work, a thermally tunable optical resonator operating in the visible wavelength range is reported, which consists of a bilayer structure composed of a thin silver layer and a dielectric coating of [Fe(HB(1,2,4‐triazol‐1‐yl)3)2] switchable spin‐crossover (SCO) molecules. White light is coupled to the resonant structure using a prism and the resulting resonance spectra are investigated as a function of the incident angle and temperature. Switching the SCO molecules from the low‐spin to the high‐spin state gives rise to a substantial blueshift of the resonances reaching up to 30 nm (associated with a reflectance modulation of up to 70%), which can be linked, through transfer‐matrix simulations, to the variation of the optical thickness of the molecular layer. Interestingly, the study demonstrated that the large thermal tunability of the device also gives rise to a photothermal nonlinearity, which can be leveraged for achieving optical limiting applications. Overall, through the present study, it is shown that molecular SCO nanomaterials can be superior to commonly used thermo‐optical switches and well‐established optical phase‐change materials for applications requiring high broadband optical transparency in the visible spectral domain.

Influence of Selective Carbon 1s Excitation on Auger-Meitner Decay in the ESCA Molecule.

Two-dimensional spectral mapping is used to visualize how resonant Auger-Meitner spectra are influenced by the site of the initial core-electron excitation and the symmetry of the core-excited state in the trifluoroethyl acetate molecule (ESCA). We observe a significant enhancement of electron yield for excitation of the COO 1s → π* and CF3 1s → σ* resonances unlike excitation at resonances involving the CH3 and CH2 sites. The CF3 1s → π* and CF3 1s → σ* resonance spectra are very different from each other, with the latter populating most valence states equally. Two complementary electronic structure calculations for the photoelectron cross section and Auger-Meitner intensity are shown to effectively reproduce the site- and state-selective nature of the resonant enhancement features. The site of the core-electron excitation and the respective final state hole locality increase the sensistivity of the photoelectron signal at specific functional group sites. This showcases resonant Auger-Meitner decay as a potentially powerful tool for selectively probing structural changes at specific functional group sites of polyatomic molecules.

Nitrogen-Doped Biochar for Enhanced Peroxymonosulfate Activation to Degrade Phenol through Both Free Radical and Direct Oxidation Based on Electron Transfer Pathways.

Nowadays, super nitrogen-doped biochar (SNBC) material has become one of the most promising metal-free catalysts for activating peroxymonosulfate (PMS) to degrade organic pollutants. To understand the evolution of SNBC properties with fabrication conditions, a variety of SNBC materials were prepared and characterized by elemental analysis, N2 adsorption-desorption, scanning electron microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. We systematically investigated the activation potential of these SNBC materials for PMS to degrade phenol. SN1BC-800 with the best catalytic performance was obtained by changing the activation temperatures and the ratio of biochar to melamine. The effects of catalyst dosage, the PMS concentration, pH, and reaction temperature on phenol degradation were studied in detail. In the presence of 0.3 g/L SN1BC-800 and 1 g/L PMS, the removal rate of 20 mg/L phenol could reach 100% within 5 min. According to electron paramagnetic resonance spectra and free radical quenching experiments, a nonfree radical pathway of phenol degradation dominated by 1O2 and electron transfer was proposed. More interestingly, the excellent catalytic performance of the SN1BC-800/PMS system is universally applicable in the degradation of other typical organic pollutants. In addition, the degradation rate of phenol is still over 80% after five reuses, which shows that the SN1BC-800 catalyst has high stability and good application prospects in environmental remediation.

Optical, thermal, FTIR, SEM-EDX and 1H NMR analysis of Chenopodium album (Bathua) powder prepared using different drying techniques

Chenopodium album (L.) is an underutilized agricultural crop consumed as a leafy vegetable in Asian countries. Although perishable and cultivated in a specific season, it contains nutrients and phytochemicals in abundance. Preservation by employing drying techniques helps in their utilization in the off-season for better food security. In the present study, Chenopodium album leaves were dried using sun, tray, and freeze drying. The different powder samples were characterized on the basis of their physicochemical, optical, and thermal properties. The water activity of powder samples ranged between 0.29 and 0.56. The highest color retention (L* value 47.21) and lowest particle size (11.5 µm) was observed in freeze dried samples. Fourier-transform infrared spectroscopy and Nuclear magnetic resonance spectra confirmed the presence of several functional groups. Thermal analysis revealed the thermal degradation of powder due heat as depicted by change of state and loss of weight. Surface morphological study indicated that powder samples were flowable and element analysis showed presence of C, O, K, Ca, Mg, P, S element in powders.

Nanocrystalline Iron Oxides with Various Average Crystallite Size Investigated Using Magnetic Resonance Method

A series of nanocrystalline iron oxide samples (M1–M5) which differ from each other in average crystallite size (from 26 to 37 nm) was studied. The raw material was nanocrystalline iron with an average crystallite size equal to 21 nm promoted with hardly reducible oxides: Al2O3, CaO, K2O (in total, max. 10 wt%). Nanocrystalline iron was subjected to oxidation with water vapor to achieve different oxidation degrees (α = 0.16–1.00). Metallic iron remaining in the samples after the oxidizing step was removed by etching. Magnetic resonance spectra of all samples were obtained at room temperature. All resonance lines were asymmetric and intense. These spectra were fitted by Lorentzian and Gaussian functions. All spectral parameters depend on the preparation method of the nanoparticles. We suppose that the Lorentz fit gives us a spectrum from larger agglomerated sizes whereas the Gaussian fit comes from much smaller magnetic centers. For the nanocrystalline samples with the largest size of iron oxide nanocrystallites, the highest value of total integrated intensity was obtained, indicating that at smaller sizes, they are more mobile in reorientation processes resulting in more settings of anti-parallel magnetic moments. The magnetic anisotropy should also increase with the increase in size of nanocrystallites.

Simulation-based approach to estimate influencing factors on acoustic resonance spectra of additively manufactured mechanical metamaterials

Acoustic Resonance Testing is a nondestructive testing method based on the analysis of eigenfrequencies of structures. While it is a well-established technique for conventionally manufactured parts, more research is needed to use the technique to quantify the properties of complex, filigree structures like additively manufactured parts. Therefore, this work examines simulation-based generation of synthetic data to estimate influencing factors caused by additive manufacturing. Using numerical eigenfrequency analysis, a systematic study of the vibration modes of a Ti6Al4V metamaterial unit cell with multistable mechanical behaviour reveals the interplay between the material properties, geometrical parameters and manufacturing-induced defects. The simulations enable the identification of specific eigenfrequencies for which the highest influence of manufacturing variations on the vibration modes are to be expected in experiments, for example, with regards to the Young’s modulus, spring width, or deflection-induced change in geometry. Frequency shift plots visualize the predicted effects of different parameters and form the basis for future guided experimental design and analysis for complex structures. The simulation-based approach allows a screening of multiple influencing factors, which is not possible experimentally. The simulation-based generation of synthetic data will contribute to the improvement of the interpretation of acoustic spectra and will extend the acoustic resonance testing for more complex structures.

The impact of mechanical recycling on the degradation of polyamide

There is currently no agreement on the degradation mechanisms for PA6 as a result of mechanical recycling. In this study, PA6 was extruded five times to simulate mechanical melt recycling process. Both virgin PA6 and the extruded PA6 were characterised to determine the predominant degradation mechanism. Melt flow rate (MFR) increases with increasing number of extrusion passes suggesting a reduction in melt viscosity due to mechanical processing. Gel permeation chromatography (GPC) results confirmed a reduction in molecular weight from 18,600 g/mol to 13,100 g/mol. Chain ends titration showed a decrease in the concentration of both the amine and carboxyl chain ends after the fifth extrusion. There were no changes to the chemical structure of the virgin PA6 and extruded PA6 observed from the Fourier transform infra-red (FTIR) and Nuclear magnetic resonance (NMR) spectra. X-ray photoelectron spectroscopy (XPS) showed a reduction in the C–N peak area supporting the scission of the N-alkylamide bond. The increase in the O=C–N peak area suggests that chain recombination via branching is possible. The shorter chains have higher mobility, and this gives rise to an increase in the crystallisation rate as seen from the differential scanning calorimeter (DSC) thermograms. The appearance of the γ phase after the fifth extrusion was identified in the DSC melting endotherms. The understanding of the degradation process of recycled PA6 will enable targeted modifications involving the incorporation of additives in the recycling process to ensure good mechanical properties in the recycled polymer.

An efficient method for the preparative isolation and purification of alkaloids from Gelsemium by using high speed counter-current chromatography and preparative HPLC

We established an efficient method using high-speed countercurrent chromatography (HSCCC) combined with preparative high-performance liquid chromatography (prep-HPLC) for isolating and purifying Gelsemium elegans (G. elegans) alkaloids. First, the two-phase solvent system composed of 1% triethylamine aqueous solution/n-hexane/ethyl acetate/ethanol (volume ratio 4:2:3:2) was employed to separate the crude extract (350 mg) using HSCCC. Subsequently, the mixture that resulted from HSCCC was further separated by Prep-HPLC, resulting in seven pure compounds including: 14-hydroxygelsenicine (1, 12.1 mg), sempervirine (2, 20.8 mg), 19-(R)-hydroxydihydrogelelsevirine (3, 10.1 mg), koumine (4, 50.5 mg), gelsemine (5, 32.2 mg), gelselvirine (6, 50.5 mg), and 11-hydroxyhumanmantenine (7, 12.5 mg). The purity of these seven compounds were 97.4, 98.9, 98.5, 99, 99.5, 96.8, and 85.5%, as determined by HPLC. The chemical structures of the seven compounds were analyzed and confirmed by electrospray ionization mass spectrometry (ESI-MS), 1H-nuclear magnetic resonance (1H NMR), and 13 C-nuclear magnetic resonance (13 C NMR) spectra. The results indicate that the HSCCC-prep-HPLC method can effectively separate the major alkaloids from the purified G. elegans, holding promising prospects for potential applications in the separation and identification of other traditional Chinese medicines.

Identifying the plateau sodium storage behavior of hard carbon through the spin state

Hard carbon has emerged as a promising anode material for rechargeable sodium-ion batteries, owing to its abundant precursor sources and remarkable reversible charge storage capacity. The key to achieving an extended sodium storage capacity lies in the plateau capacity largely associated with the closed-pore structure, yet a comprehensive understanding in this area remains incomplete. In our study, we utilized electron paramagnetic resonance (EPR) spectra to discern the spin state of unpaired electrons within hard carbon materials, enabling the identification of sodium storage plateau regions. Hard carbon anodes with plateau capacity predominantly exhibit delocalized spins, evident in the EPR spectrum by limited spin density and a linewidth exceeding 100 G. These spins originate from the extended aromatic structure within small-sized but curved nano-graphite and the closed-pore walls, which are crucial for plateau capacity. Conversely, hard carbon anodes exclusively possessing slope capacity are characterized by localized spins, presenting a typical narrow and intense Lorentzian EPR signal. These localized spins arise from the edge defects of the nano-graphite structure, serving as favourable sites for sodium adsorption. Our development of a methodology to discern hard carbon plateau capacity behavior based on EPR spectra presents a facile and rapid approach for advancing high-performance hard carbon materials.

Replicating Spectral Baseline for Unambiguous Frequency Locking in Resonant Sensors.

Electrothermal piezoresistive resonant cantilever sensors have been fabricated with embedded actuating (heating resistor) and sensing (piezo resistors) parts, with the latter configured in a Wheatstone bridge circuit. Due to the close spacing between these two elements, a direct thermal parasitic effect on the resonant sensor during the actuating-sensing process leads to asymmetric amplitude and reversing phase spectral responses. Such a condition affects the precise determination of the cantilever's resonant frequency, f0. Moreover, in the context of phase-locked loop-based (PLL) resonance tracking, a reversing phase spectral response hinders the resonance locking due to its ambiguity. In this work, a replica of the baseline spectral was applied to remove the thermal parasitic effect on the resonance spectra of the cantilever sensor, and its capability was simulated through mathematical analysis. This replica spectral was subtracted from the parasitized spectral using a particular calculation, resulting in optimized spectral responses. An assessment using cigarette smoke particles performed a desired spectral shifting into symmetrical amplitude shapes and monotonic phase transitions, subsequently allowing for real-time PLL-based frequency tracking.